Standard Operating Procedure for Review of Instrument Calibration Logs in BA/BE Studies
| Department | BA-BE Studies |
|---|---|
| SOP No. | SOP/BA-BE/200/2025 |
| Supersedes | SOP/BA-BE/200/2022 |
| Page No. | Page 1 of 9 |
| Issue Date | 17/04/2025 |
| Effective Date | 20/04/2025 |
| Review Date | 17/04/2026 |
1. Purpose
To define the procedure for reviewing instrument calibration logs to ensure that all analytical equipment used in bioanalytical studies for BA/BE trials is accurately calibrated and meets performance requirements prior to use.
2. Scope
This SOP applies to all calibration logs of critical analytical instruments including HPLC, LC-MS/MS, balances, pH meters, and centrifuges used in the bioanalytical laboratory for BA/BE
studies.
3. Responsibilities
- Analyst/Technician: Performs and records calibration data in the logbook.
- QA Officer: Verifies calibration completeness and compliance with SOP.
- Lab Supervisor: Reviews calibration data for validity and signs off.
4. Accountability
The Head of the Bioanalytical Department is accountable for ensuring that no analytical activity is performed using uncalibrated or non-compliant equipment.
5. Procedure
5.1 Calibration Log Maintenance
- Each instrument shall have a dedicated calibration logbook or electronic log (Annexure-1).
- Logbook entries must include:
- Calibration date
- Parameters checked
- Observed values
- Acceptance range
- Deviation (if any)
- Initials and signature
5.2 Review Frequency
- Review instrument calibration logs:
- Monthly for high-frequency use instruments (e.g., LC-MS/MS)
- Quarterly for support equipment (e.g., balances, pH meters)
- Conduct additional reviews:
- Before study initiation
- During audits or inspections
- Following any instrument malfunction
5.3 Review Process
- Cross-check the calibration dates against due dates and SOP schedules.
- Verify:
- Calibration was performed within schedule
- All parameters meet acceptance criteria
- No data overwriting or missing entries
- Highlight discrepancies and incomplete calibrations in the Calibration Review Summary (Annexure-2).
5.4 Handling Deviations
- If calibration is overdue:
- Label equipment as “Out of Service”
- Inform the Lab Head and QA
- Prevent usage until recalibrated
- If calibration results are out of specification:
- Stop equipment use
- Log deviation in Deviation Register
- Investigate root cause and initiate corrective actions
5.5 Documentation
- Ensure every review entry includes:
- Reviewer name
- Date of review
- Comments
- Signature
- Maintain reviewed logs in the equipment calibration file for 5 years.
6. Abbreviations
- BA/BE: Bioavailability/Bioequivalence
- SOP: Standard Operating Procedure
- QA: Quality Assurance
- HPLC: High-Performance Liquid Chromatography
- LC-MS/MS: Liquid Chromatography with Tandem Mass Spectrometry
7. Documents
- Instrument Calibration Logbook – Annexure-1
- Calibration Review Summary – Annexure-2
8. References
- ICH Q9: Quality Risk Management
- OECD GLP Principles
- 21 CFR Part 11 – Electronic Records & Signatures
9. SOP Version
Version: 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | |||
| Designation | |||
| Department |
11. Annexures
Annexure-1: Instrument Calibration Logbook
| Instrument ID | Date | Parameter | Observed Value | Acceptance Range | Performed By |
|---|---|---|---|---|---|
| LCMS-03 | 15/03/2025 | Retention Time | 2.52 min | 2.5 ± 0.2 | Ajay Verma |
Annexure-2: Calibration Review Summary
| Date | Instrument ID | Reviewer | Compliance | Remarks |
|---|---|---|---|---|
| 17/04/2025 | LCMS-03 | Sunita Reddy | Yes | All parameters within limits |
Revision History:
| Revision Date | Revision No. | Details | Reason | Approved By |
|---|---|---|---|---|
| 01/01/2022 | 1.0 | Initial SOP | New implementation | QA Head |
| 17/04/2025 | 2.0 | Updated review frequency and deviation control steps | Audit recommendation | QA Head |